• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.7 no.1
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• pp.49-59
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• 1997

This study was performed to analyze the purity of technical grade ${\alpha}$-naphthylamine, to establish optimal analytical condition of ${\alpha}$-naphthylamine in urine and to determine the urine sample of workers exposed to ${\alpha}$-naphthylamine. The purity of technical grade ${\alpha}$-naphthylamine were $96.5{\pm}2.38%$, $94.1{\pm}0.97%$, $97.0{\pm}0.02%$ by gas chromatography-mass selective detector. To analyze ${\alpha}$-naphthylamine in urine, high performance liquid chromatography-electrochemical detector and gas chromatography-electron capture detector operating conditions have been optimized by preliminary expriment. In high performance liquid chromatography-electrochemical detector, the mobile phase was consisted of acetonitrile(35%) and water(65%), and the flow rate was maintained at 1.0ml per minute. Optimal detective condition was 9.0V(10nA/V) of electrochemical detector. The recovery of sep-pak treatment method was highly estimated as pretreatment of ${\alpha}$-naphthylamine in urine. The free amine was isolated by gas chromatography-electron capture detector after basic hydrosis, sep-pak treatment, toluene elution and HFBA(heptafluoro-butyric anhydride) derivatization of urine. The recovery of ${\alpha}$-naphthylamine in urine was $98.73{\pm}3.29%$ by gas chromatography-electron capture detector. The sensitivity was more higher than that of high performance liquid chromatography-electrochemical detector. Urinary ${\alpha}$-naphthylamine was detected in only one worker among nine workers. The level of ${\alpha}$-naphthylamine in urine was 6.42 ng/ml.

• Journal of Food Hygiene and Safety
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• v.16 no.1
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• pp.61-65
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• 2001

To investigate the optimum condition of 3-monochloro-1, 2-propanediol(MCPD) analysis, gas chromatography with electron capture detector was used. Determination of MCPD derivatized with phenylboric acid was more effective than that of underivatized MCPD. In derivatization of MCPD with phenyl boric acid, there were no significantly different between boiling for 2min at 9$0^{\circ}C$ and vortexing for 5min at room temperature. Extrelut column was suitable for extraction of MCPD diluted in 20% NaCl solution and recovery rates were higher than direct extraction of MCPD with ethyl acetate. But, the method of direct extraction of MCPD with ethyl acetate was useful for rapid ants qualitative analysis. The sample extracted in soysauce(ganjang) was derivatized with phenylboric acid and analyzed by gas chromatography-mass selective detector. That was confirmed as MCPD-phenylboronate.

• Journal of the Korean Society for Precision Engineering
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• v.25 no.4
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• pp.53-60
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• 2008

Electron detectors used in scanning electron microscope accept electrons emitted from the specimen and convert them to an electrical signal that, after amplification, is used to modulate the gray-level intensities on a cathode ray tube, producing an image of the specimen. Electron detector is one of the key components dominating the performance of scanning electron microscope so that the development of electron detectors having high performance is indispensable to acquire high quality images using scanning electron microscope. In this paper, we designed and manufactured an electron detector and conducted a couple of image capture experiments using it. In particular, scintillator which generates light photons when it is struck by high-energy electrons was manufactured and experimental studies on the optimization of manufacturing condition was carried out. From experiments to evaluate the performance of our detector, it was verified that the performance of our detector is equivalent to or better than that of the conventional one.

• Food Science and Biotechnology
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• v.15 no.6
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• pp.959-966
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• 2006

The electron-capture detector (ECD) of gas chromatographs (GC) has been used widely in pesticide analysis. However, as ECD relies on radioactive material, it is troublesome to purchase and maintain. Therefore, potent replacements for ECD were investigated. A Pulsed-discharge detector (PDD) for ECD was tested and the analytical results of PDD (ECD mode), ${\mu}ECD$, and nitrogen-phosphorus detector (NPD) were compared for 107 pesticides including organochroline, organophosphorus, pyrethroids etc. The number of pesticides identified at the lowest limit of detection (LOD) was 36, 29, and 2 for PDD, ${\mu}ECD$, and NPD, respectively. The remaining pesticides showed same response to PDD and ${\mu}ECD$. The GC-PDD analysis of pesticides spiked into representative agricultural products (brown rice, spinach, and mandarin oranges) also showed good and/or equivalent recoveries using $GC-{\mu}ECD$.

• Journal of Environmental Science International
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• v.6 no.4
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• pp.385-389
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• 1997

Pesticide residues were extracted with 70% acetone and transferred to dichloromethane. Extracts were applied to open-column chromatography with florisil and alumina-N. The final extract was analyzed by gas chromatography with electron-capture detector(GC /ECD) and nitrogen-phosphorus detector(GC/NPD). Recoveries of the 17 organochlorine pegticides were ranged from 60.8 to 84.9% and those of 15 organophosphate pesticides, from 70.5% to 100.0%(except phosmet and azlnphos-methyls. The minimum detectable levels of this analytical method were low(0.021-0.058mg/kg).

• 한국생물공학회:학술대회논문집
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• 2003.04a
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• pp.729-729
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• 2003

• Environmental Analysis Health and Toxicology
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• v.17 no.2
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• pp.117-123
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• 2002

A gas chromatographic method for the determination of airborne formaldehyde was established. In order to be highly detectable with the electron capture detector, formaldehyde was derivatized to its pentafluorobenzyl oxime form by reacting with O- (2,3,4,5,6- pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA) at pH of 4.6 and temperature of 50$^{\circ}C$ for 1 hour. Air samples were collected into a Tedlar$\^$(R)/ bag followed by transferring into water contained in two impingers in series. Collection efficiency in the front trap was higher than 90％. Measurement of selected indoor and outdoor air samples showed higher formaldehyde concentrations in indoor air environments and the importance of ventilation for reducing indoor pollution.

• Proceedings of the Korean Environmental Sciences Society Conference
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• 1997.10a
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• pp.37-39
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• 1997

Pesticide residues were extracted with 70% acetone and transferred to dichloromethane. Extracts were applied to open-column chromatography with florisil and alumina-N, The final extract was analyzed by gas chromatography with electron-capture detector(GC/ECD) and nitrogen-phosphorus detector(GC/NPD). Recoveries of the 17 organochlorine pesticides were ranged from 60.8 to 84.9% and those of 15 organophosphorus pesticides, from 70.5 to 100.0%(except phosmet and azinphos-methyl). The minimum detectable levels of this analytical method were low (0.021-0.058 mg/kg).

• Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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• 2005.04a
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• pp.199-201
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• 2005

This paper describes a simple procedure for the quantitative analysis of 7 PCBs (polychlorinated biphenyls) in soils on the waste reclaimed land, The procedure involved sample clean up using silicagel column, acetonitrile partition and sulfuric acid procedures. The instrumental technique is applied GC/PDD(gas chromatography/pulsed discharge detector) and GC/ECD(gas chromatography/electron capture detector). Concentration of $sub-{\mu}g/g$ level was attainable with 20g soils on the waste reclaimed land.

• Analytical Science and Technology
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• v.12 no.5
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• pp.408-414
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• 1999

A selective and sensitive method for the derivatization of total homocysteine (Hcy) and the related compounds in plasma by gas chromatograph (GC)-electron capture detector (ECD) has been developed. To determine total homocysteine, cysteine (Cys), and methionine (Met) in human plasma using GC-ECD, analytes were reduced and converted into their N(O,S)-ethylearbonyl pentafluoropropyl (PFP) ester by derivatization with ethyl chloroformate and pentafluoropropyl alcohol (PFP-OH) in plasma. The best derivatizing agent N(O,S)-ethyl carbonyl PFP ester, was chosen by comparing the sensitivity of derivatized analysis in GC-ECD. The derivatized analytes in plasma were extracted by chloroform, and subsequently back-extracted with hexane and analyzed by GC-ECD. The calibration carves ($R^2$ > 0.990) were linear over the range $5-50{\mu}mol/L$ of Hcy and Met, $40-400{\mu}mol/L$ of Cys spiked in plasma. The detection limit observed by the established method was below $0.5{\mu}mol/L$. This method is highly sensitive and specific in the analysis of Hcy, Cys, and Met. Therefore, we suggest that this method is appropriate in the analysis of trace concentration of Hcy, Cys, and Met in biological fluids.